Hydrothermal Synthesis,crystal Structure And Properties On Novel Aminopyridine And 1, 10-phenanthroline Polyoxometalates Complexes

Eight (1-8) novel polyoxometalates complexes crystals have been synthesized under hydrothermal conditions and structurally characterized by single-crystal X-ray diffraction, IR, UV/Vis and TG-DTA.Cyclic voltammetric behavior of complex 1 and 2 have been studied in solution.Two novel polyoxometalates complexes: (C₅H₇N₂)3(AsMo₁₂O₄₀)·- 2(C₅H₆N₂)·1.5H₂O 1 and (C₅H₇N₂)2(PMo₁₂O₄₀)·3(C₅H₆N₂)·0.5(C₄H₈N₄)·- 0.5H₂O 2 have been synthesized with the ligand 2-aminopyridine. Complex 1 crystallizes in monoclinic, space group P2(1)/n, with the cell parameters of a=13.310(3)A, b=22.399(5)A, c=19.820(4)A,β=99.99(3)°, V=5819(2)A³, Z=4, R_gt(F)=0.0477,ωR_ref(F²)=0.1376, S=1.075. Complex 2 crystallizes in monoclinic, space group P2(1)/n, with the cell parameters of a=13.3281(6)A, b=22.4452(10)A, c=21.9954(9)A,β=116.007(2)°, V=5913.7(5)A³, Z=2, R_gt(F)=0.0430,ωR_ref(F²)=0.1266, S=1.041. Complex 1 and 2 are linked to supramolecular structure via hydrogen-bonding between 2-aminopyridine and polyoxoanion. CV indicate that Complex 1 and 2 have good redox stability. Complex 1 and 2 posssess high thermal stability. The catalytic performance measurement results showed that over the 0.15g compound, the acetone with concentration 5.3 g·m-3 and velocity of flow 2.5 mL·min-1 can be completely eliminated under 150℃, it is a potential catalyst.Two novel polyoxometalates complexes: (C₅H₇N₂)2H(CrMo₆Cl₆O₁₈)-·4H₂O 3 and (C₅H₇N₂)5(AsMo₁₂O₄₀)·0.5(C₅H₆N₂)·H₂O 4 have been synthesized with the ligand 3-aminopyridine. Complex 3 crystallizes in triclinic, space group P-1, with the cell parameters of a=7.8482(8)A, b=10.1800(10)A, c=10.4103(10)A,α=88.031(3)°,β=78.308(2)°,γ=88.842(3)°, V=1386.62A³, Z=1, R_gt(F)=0.0659,ωR_ref(F²)=0.1936, S=1.077. Complex 4 crystallizes in monoclinic, space group P2(1)/n, with the cell parameters of a=13.3820(12)A, b=22.542(2)A, c=19.848(2)A,β=100.27(3)°, V=5891.2(10)A³, Z=4, R_gt(F)=0.0538,ωR_ref(F²)=0.1557, S=1.088. Complex 3 and 4 are linked to supramolecular structure via hydrogen-bonding between 3-aminopyridine and polyoxoanion. Complex 3 and 4 posssess high thermal stability.Two novel polyoxometalates complexes: [CrMo₆(OH)₆O₁₈]·2(C₅H₆N₂)-·3H₂O 5 and (C₅H₇N₂)3(PMo₁₂O₄₀)·2(C₅H₆N₂)·0.5(C₄H₆N₃) 6 have been synthesized with the ligand 4-aminopyridine. Complex 5 crystallizes in triclinic, space group P-1, with the cell parameters of a=7.8564(6)A, b=9.9094(7)A, c=10.2144(9)A,α=89.063(2)°,β= 78.0460(10)°,γ=86.273 (3)°, V=776.32(11)A³, Z=2, R_gt(F)=0.0447,ωR_ref(F²)=0.1297, S=1.139. Complex 6 crystallizes in monoclinic, space group C2/c, with the cell parameters of a=14.2722(10)A, b=21.9896(16)A, c=36.027(2)A,β=100.410 (3)°, V=11120.6(13)A³, Z=4, R_gt(F)=0.0357,ωR_ref(F²)=0.0965, S=1.042. Complex 5 is linked to supramolecular structure via strong hydrogen-bonding between coordinated water molecular and polyoxoanion. Complex 6 is linked to supramolecular structure via hydrogen-bonding between 4-aminopyridine and polyoxoanion. Complex 5 and 6 posssess high thermal stability.Two novel polyoxometalates complexes: [Cu(H₂O)2(phen)(Mo₄O₁₃)] 7 and [Fe(phen)₃]₂(PMo10Vâ…¤3Vâ…£O44)·DMF 8 have been synthesized with the ligand 1,10-phenanthroline. Complex 7 crystallizes in triclinic, space group P-1, with the cell parameters of a=8.5794(9)A, b=10.0961(9)A, c=12.6883 (12)A,α=86.243(2)°,β=83.642(2)°,γ=67.7510(10)°, V=1010.63(17)A³, Z=2, R_gt(F)=0.0341,ωR_ref(F²) =0.0956, S=1.070. Complex 8 crystallizes in monoclinic, space group C2/c, with the cell parameters of a=14.1341(4)A, b=18.3509(6)A, c=19.6763(7)A,α=83.2250(10)°,β=69.7870(10)°,γ=87.0210(10)°, V=4755.4(3)A³, Z=1, R_gt(F)=0.0459,ωR_ref(F²) =0.1079, S=1.016. Complex 7 and 8 are linked to supramolecular structure via hydrogen-bonding between 1,10-phenanthroline and polyoxoanion. Complex 7 and 8 posssess high thermal stability.